Method of manufacturing dulled artificial products of viscose



' substance.

Patented July 28,1936

G I. z

VISCOS Cayser, Rorschach, Swit-- a, i yo Loch, oenield Rorschach. Switserland application may A25. in

This invention reiatesto methods of turing dulled or matted products oi It is known to make dulled or matted products 01 viscose having amaximum n 1 v. capacity in 5 such a mariner that the viscose is mixed with inorganic plgments which, when the viscose is precipitated, remaintin the and thus impart to the thread or film the desired lucid glassy aspect and render it dull and opaque. 1g As, for makineany I cose must be, extruded through extremely minute apertures, it is required to apply the pigments in manufacsuch a fine state. and to divide them throughout the mass of the viscose in tionftha't' the minute apertures are not clogged during the spinning process. Though it is possible to grind pigments such a fine distrlbu regard to degree of fineness I to be obtained, these so flneparticles, for example of titanium dioxide,

which compound is preferably applied for dulling tinging capacity, stick purposes due to i to'each other so its high to speak in the iormoi viscous conglomerates so fast that distributin the compound through the viscid viscose is extremely diilicult and spinninga viscose having dry titanium dioxide admixed thereto by" lmeading is altogether impossible.

1 For this reason, it has already-been proposed to pass the viscose prior to the spinning prom through filter presses which are lagged with Y densely woven fabrics with a viewto attaining the required degree of distribution by the filtering operation. But

about thedesired result as the presses become clogged and thus a portion of the titanium diox ide is kept back, so that the viscose, which passes through the filter press first, contains, depending -on the degree oipermeability 'oithe press, a higher, percentage amount ortltanium dioxide than the viscose passing through later. This results in noneuniiormities even it the viscose he i subsequently homogenized once more, as'every individual charge of a number of consecutive 4.5 charges differs from the others and consequently a great varietyoi difierent degrees oi dulling oi the spun threads ensues, due to the extraordinary eificiency oi the titanium dioxide, slight differences in the e from this, a con 1 tion is impossible also due to the press s becoming clogged after a short time, being-frequently interrupted- "In an endeavour to avoid'this deficiency, it has alreadybeenpropcsedtoadmlxtotheviscosein addition to titanium such as ior examp r facilitating the filtration. At the same time at tempts were. ma e to obtain a .9!

dullinsbymeansotthisaddltiom,

product unchanged kind of products, the vis-- in dry condition to a nearly colloidal state which satisfies the requirements in stirring or also these methods tailed to even with. but specific content of this tinuedproducthe operation thus fdioxide other with -a vlew to;

Fele A.

lot. inc-4o) The filtering process is, however, not-.obviated by this measure and thus this method is unreliable in the same-way as the previously mentioned one. Similar dimculties are encountered asin the method wherein no additional ingredients are used,-as also here the presses are quickly obstructed. Therefore it is necessary to homogenize the mass once more after the filtering, in order to obtain auniform dulling effect throughout, but even then the disadvantage ensues that Y thevarious eharges are of difierent dulling ef- Though by adding petroleum to viscose it is feasible to obtain a drilling effect, the presence of titanium'dioxide prevents this eiiect from showing up, so that the said addition is useless in this respect.

Thus it will beseen that by means of this known method it impossible to obtain either continuity of production nor special effects of 20 culling. Moreover, the relatively high percentage amountof' petroleumis detrimental to the strength of the spun viscose threads.

Again, it has. also been proposed to mix th titanium dioxidewith liquids prior to adding it to the viscose: with a view to facilitating the. f homogenizing of the viscose mixture.

As liquids iorthis purpose, for example, on the one hand water or solving agents respectively, for the'mass to be spun have been recommended and on the other'hand oils, such as linseed oil, olive oil and the like. With the aid of these means it is intended to homogenize the pigment in a ballmill. Experience has now shown that by the addition of water merely a suspension ensues and thus the formation of va. homogeneous mass is prevented. with the aid oi oils, as lin- 'seed and olive oils, a sufliciently homogeneous mixture is obtained only if considerable amounts oioil'are admixed. Additions of Turkey red'oil which is recommended asa dispersing agent have no improving-effect.

Water and other liquids dissolving the, viscose are advantageous for use as carriers for the pigment in so far as these liquids separate from the thread during the spinning process and thus do not cause dulling of the viscose and should be expected to assist in furnishings thread which is stronger than one containing in addition to the pigment, for example titanium dioxide, still other foreign substances.- It is, however, a'surprising fact that, when; such substances are used, the spinning process does nht always take a satisfactory course even in the event of the. titanium I dioxide having apparently been uniformly admixed, and the strength or the spun threads does up "to expectations, while the 'All of this is due to theconto be met in endeavouring .to

- not always .come .yieldals too 'small.

siderable dimculty obtain the requisite ma uniformity of dis tribution of the individual-particles. Relatively large quantities of the said oils are of the high percentage amount of foreign substances. By the application of titanium dioxide alone the fibres are weakened, and due to the presence of oil as a subsidiary means the strength of the material is further decreased, so that the quality of the silk is naturally lessened. More- 7 over, thismethod has the disadvantage inherent l5 thereto that the oils are liable to change texture dueto their saponifiability and thus the quality or the silk, containing such oils. gradually decreases when the silkis stored. f

i It is, however, impossible to use for this method substances such as for example liquid parafiine, petroleum, -benzine, pinene, benzene, tetraline, decaline or the like which substances as such have no detrimental eifect on the finished prod not, as these substances were required to be added in such large percentage amounts that a thread the addition of Turkey red oil would not help for changing these percentage amounts.

Thus, of these substances a weight almost three times as large asthat of the'equivalent amount' 5 the start. In most cases, namely. it is impossible It was now found asa surprising fact that just the substances mentioned above. which mix 40 with titaniumdioxide only with'diiiiculty and in 1' The distribution thus obtained is so fine that 'anysort o f filtration for improving the (homogeneity. as'p'rescribed by most of the methods is dlspe conditions are smmuchinore surprising as the 55 same method when applied tofatty oils fails to produce the same eifect.

a In mixing titan'iumdioxide with diil'erent subi stances. in the proportion -of 1' :1 the. following 3 effects are obtained:

Without addition oilul nomad minim with o! an] h oil M natednii raloiia dd c d.

1. Do. Semi-liquid mass: Var liquid mess. I

Do. Do. 1

From this tabulation it follows that just the v oils that were hitherto recommended for producing pigment pastes for the manufacture of matted used with, Th s Isulphonated mineral oil,:

' silk have no peculiar eifects when sulphonated mineral oil isadmixed, but that the substances which can not be used alone and which had so far not been used at all behave beyond expectation in an entirely contrary manner. 5

The sulphonated mineral oil admixed to these substances eii'ects upon stirring readily and quickly a perfect dispersion with the pigmentso that a smooth mass-is obtained If the stirringv is continued-for a length of time insuflicient for 1:)

mass to stand, even if sulphonated 'mineral oil be admixed. The high fluidity and smoothness of the mass is due to the fact that conglomerates 29 of particles are no longer present but that the whole mass consists of a uniform distribution of individual particles. v

Owing to the dispersiveness of the sulphonated mineral oil aid in spite of the small quantity of oil present every minute particle of titaniumdioxide is separately enveloped in a covering film of oil and only after the formation of these films, whereby the oil acts as a support,- it is possible to admixthe titaniumdioxide to the viscose in a perifectly uniform manner.

When this. mass to which the sulphonated mineral oil is admixed is added to the viscose, the

mass on stirring divides through the viscose rapidly to give it a smooth appearance contrary to a mass which is prepared from other oils with granular aspect which disappears only after con siderable stirring combined with filtering, but 40 which may nevertheless cause sedimentation during the time required for the vi'sco'se'to stand for the air'to escape therefrom and during the I any viscose emulsified with the substances previphonated mineml il was'added to thesesubstances; presents even after only a brief mixing any. further provisions.

Due to the extraordinary dispersiyeness of the The method according to this invention has the enormous-advantage inherent "thereto that by when applied to titanium directly were of but a slight effect, is avoided and consequently the percentage amount of titanium to be added can be increased to have its full effect.

Therefore, by applying the method according to the invention not only safety of operation in manufacturing dulled titanium silk is warranted, but also the production of threads presenting an aspect from a dull silvery lustre to a lustre specifically characteristic for cotton without, however, being accompanied by the slightest surface sheen due to the relatively large amount of titaniumdioxide which can be incorporated in the viscose without difficulty. Furthermore, the manufacture of a product of a high quality is ensured which is of normal strength and the degree of dulling of which can be maintained constant uniformly throughout. Moreover; the auxiliary substances entering into question are cheap and the quantities necessitated small. Waste losses of material which unavoidably arise in filtering are avoided.

Example 1 120 grams of titaniumdioxide are mixed with grams of liquid parafilne to which 10 grams of sulphonated mineral oil were added, and mixed intimately. The paste obtained is emulsified with kilograms of viscose of a requisite degree of maturation and homogenized. After the air has been caused to escape spun in usual manner.

A slightly dulled thread results.

Example 2 grams of titanium dioxide are intimately mixed together with 50 grams of fluid paraffine to which 10 grams of 'sulphonated mineral oil were added, and mixed intimately. The paste obtained is emulsified with 40 kilograms of viscose of the requisite degree of maturation and homogenized. After the air has been caused to escape the viscose is spun in usual manner.

the viscose is A highly dulled thread results.

In a similar manner viscose emulsions as described can be worked into films.

We do not limit ourselves to the particular size, shape, number or arrangement of parts as shown and described, all of which may be varied without going beyond the scope of our invention as shown, described and claimed.

What we claim is:

l. in a process for the production of low luster artificial compositions from viscose in which titanium dioxide is used as a delustering agent, the steps comprising intimately admixing T102 with asubstance selected from the group consisting of liquid parafline, benzene, pinene, tetraline, and decaline, in the presence of a sulfonated mineral oil and thereafter emulsifying and homogenizing the mixture with viscose.

2. Process for the production of low luster artificial compositions from viscose in which TiO2 is used as a delustering agent, the steps comprising intimately admixing the TiOz with a liquid paraifine in the presence of sulfonated mineral oil, and thereafter emulsifying and homogenizing the mixture so produced with viscose.

3: Process for the production of low luster artificial compositions from viscose in which T102 is used as a delustering agent, the steps comprising intimately admixing the TiOz with a benzolin the presence of the sulfonated mineral oil, and' thereafter emulsifying and homogenizing the mixture so produced with viscose.

4. Process for the production of low luster artificial compositions from viscose TiOz is used as a delustering agent, the steps comprising intimately admixing the TiOz with a pinene in the presence of sulfonated mineral oil,

' and thereafter emulsifying and homogenizing the mixture so produced with viscose.

Q KURT WITTE.

HANS cAxsEa. 

